CN105030891B - preparation method and application of dracocephalum heterophyllum flavonoid component - Google Patents
preparation method and application of dracocephalum heterophyllum flavonoid component Download PDFInfo
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Abstract
The invention relates to a preparation method of an dracocephalum heterophyllum flavonoid component, which comprises the following steps: the method comprises the following steps: drying the dracocephalum heterophyllum benth in the shade, crushing, extracting with ethanol or methanol solution with a certain volume concentration, and drying the extract under reduced pressure to obtain the dracocephalum heterophyllum benth plant alcohol extract. Secondly, liquid and liquid distribution and enrichment: dispersing, extracting and drying the dracocephalum heterophyllum plant alcohol extract under reduced pressure to obtain medium-polarity component parts of dracocephalum heterophyllum; removing impurities by using microporous resin: dissolving the medium-polarity component parts of the dracocephalum heterophyllum benth, filtering, separating by a microporous resin column, eluting, and collecting the eluate; drying the eluate under reduced pressure to obtain yellow crude product of flavonoid component of Dracocephalum heterophyllum; fourth, silica gel column chromatography separation: and (3) separating and eluting the crude product of the flavonoid component of the dracocephalum heterophyllum benth by silica gel column chromatography, detecting by adopting thin-layer chromatography, merging and collecting fractions with Rf value of 0.1-0.8, and drying the fractions under reduced pressure to obtain the yellow powdery flavonoid component of the dracocephalum heterophyllum benth. The invention has simple process and easy scale production. The invention also discloses application of the dracocephalum heterophyllum flavonoid component in preparing anti-hepatitis virus drugs or health-care foods.
Description
Technical Field
The invention relates to a preparation method of a flavonoid component, in particular to a preparation method and application of an dracocephalum heterophyllum flavonoid component.
Background
Dracocephalum heterophyllum Labiatae DracocephalumThe Dracocephalum heterophyllum Benth (Dracocephalus heterophyllum Benth) is a plant of the genus Dracocephalum of the family Labiatae (Labiatae) and is mainly distributed in the temperate zone of Asia. The plant is widely used in folk, and has effects of suppressing hyperactive liver, clearing heat, and treating hypertension, lymphadenitis, and cough due to lung heat. Modern researches show that the chemical components in the dracocephalum heterophyllum benth mainly comprise phenylpropanoids, flavonoids and terpenoids, wherein the flavonoid compounds are well known for the remarkable activities of antioxidation, cardiovascular and cerebrovascular disease treatment, tumor resistance and virus resistance.
at present, no document is reported on the preparation of the antiviral active flavonoid component from the dracocephalum heterophyllum benth, and a Chinese patent (CN 103070916B) reports that the flavonoid component for treating hypertension in the dracocephalum heterophyllum benth is enriched by adopting the processes of ethanol extraction and macroporous resin treatment, however, no document is reported on the research of the preparation method for obtaining the large-scale antiviral active flavonoid component from the dracocephalum heterophyllum benth so far.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for preparing the flavonoid component of the dracocephalum heterophyllum benth, which has simple process and is easy to scale.
The invention also aims to provide the application of the flavonoid component.
In order to solve the problems, the preparation method of the flavonoid component of the dracocephalum heterophyllum comprises the following steps:
First extraction
Drying and crushing the dracocephalum heterophyllum benth plant in the shade, adding an ethanol or methanol solution with the volume concentration of 95% and the mass of 8-20 times of that of the dracocephalum heterophyllum benth plant, soaking for 10-15 hours, heating and refluxing for 2-4 times at 80-90 ℃, extracting for 3 hours each time to obtain an extracting solution, and drying the extracting solution under reduced pressure to obtain a paste, namely the dracocephalum heterophyllum benth plant alcohol extract.
Secondly, liquid and liquid distribution and enrichment:
Dispersing the dracocephalum heterophyllum plant alcohol extract by using 30-50 times of analytical pure water by mass to obtain dispersion liquid, extracting the dispersion liquid for 3 times by using 30-50 times of ethyl acetate by volume, and combining to obtain ethyl acetate extract; the ethyl acetate extract is dried under reduced pressure to obtain the medium-polarity component part of the dracocephalum heterophyllum;
removing impurities by using microporous resin:
Dissolving the medium-polarity component parts of the dracocephalum heterophyllum benth with a methanol solution with the mass of 5-10 times and the volume fraction of 80-90%, filtering to obtain a filtrate, separating the filtrate on a microporous resin column, eluting with a methanol solution with the volume fraction of 3-5 times and the volume fraction of 80-90%, and collecting the eluate of the methanol solution with the volume fraction of 80-90%; decompressing and drying the eluate of the 80-90% methanol solution to obtain a yellow crude product of the flavonoid component of the dracocephalum heterophyllum; the proportion of the medium-polarity component part of the dracocephalum heterophyllum benth to the microporous resin is 1 g: 30 mL;
fourth, silica gel column chromatography separation:
Separating the crude flavonoid component of the dracocephalum heterophyllum benth by silica gel column chromatography, eluting with a chloroform-methanol mixed solvent with the volume of 5-10 times of the column volume, collecting fractions according to 500-1000 mL of each fraction, and detecting by adopting thin-layer chromatography, wherein a developing agent is chloroform and methanol, and the ratio of chloroform to methanol is 5: 5, the color developing agent is concentrated sulfuric acid ethanol solution with volume concentration of 10%, fractions with Rf value of 0.1-0.8 are merged and collected, and the fractions are dried under reduced pressure to obtain yellow powdery flavonoid components of the dracocephalum heterophyllum benth.
The reduced pressure drying condition is that the vacuum degree is 0.06-0.09 MPa and the temperature is 50-70 ℃.
The microporous resin in the step three is an HP20SS type resin column or an MCI type resin column.
The size of the silica gel column in the step four is 40 mm-80 mm multiplied by 60 cm-100 cm.
The chloroform-methanol mixed solvent in the step four is a mixture of chloroform and methanol in a ratio of 7: 3-3: 7 by volume ratio.
The application of the dracocephalum heterophyllum flavonoid component prepared by the preparation method of the dracocephalum heterophyllum flavonoid component in preparing anti-hepatitis virus medicines or health-care foods is characterized in that: the flavonoid component of the dracocephalum heterophyllum benth can be used as an effective component to prepare various anti-hepatitis virus medicinal preparations with any pharmaceutically acceptable carrier by a conventional method, or can be used as an effective component to prepare various health-care foods with any pharmaceutically acceptable carrier by a conventional method.
compared with the prior art, the invention has the following advantages:
1. The invention adopts a liquid-liquid distribution method to enrich the parts of the polar components such as the dracocephalum heterophyllum, and the solvent has low price, can be regenerated and recycled, and is easy for large-scale production.
2. The method adopts the microporous resin to remove impurities, can efficiently remove the pigment in the sample, can regenerate and recycle the resin column, has low average price and is easy for scale production.
3. The method adopts silica gel column chromatography separation, can directly separate the flavonoid component from the low-polarity component in the dracocephalum heterophyllum benth, and simultaneously removes part of high-polarity impurities.
4. the invention has low requirement on raw materials, can be used as common or wild raw materials in the market, and is easy to prepare in batches.
5. The method has the advantages of simple process, good repeatability and stable and controllable quality, and the obtained dracocephalum heterophyllum flavonoid components are sequentially judged to mainly contain apigenin, naringenin and other flavonoid compounds through two-dimensional preparative chromatographic separation and purification and NMR hydrogen spectrum and carbon spectrum analysis.
6. The flavonoid component of the dracocephalum heterophyllum benth obtained by the invention has good effect of resisting hepatitis virus through tests.
The method simulates the pathological liver cell necrosis caused by virus-induced autoimmune disorder in viral hepatitis by using the sword bean protease to cause excessive immune reaction of a liver immune system to the liver and cause liver tissue damage. In the pathological model, the functions of the flavonoid component medicines of the dracocephalum heterophyllum are researched, the transaminase value index change of a control group and a balb/c mouse flavonoid component medicine group of the dracocephalum heterophyllum is detected to judge the medicine effect of the mixed component, and the in vivo experiment groups are shown in table 1:
TABLE 1
The conclusion is that: the flavonoid component of the dracocephalum heterophyllum benth can remarkably treat liver injury caused by the autoimmune reaction of an organism. See figure 1 for details.
Drawings
the following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
FIG. 1 shows the screening results of the anti-hepatitis virus activity of the flavonoid component of Dracocephalum heterophyllum Benth.
Detailed Description
embodiment 1 a method for preparing flavonoid components from dracocephalum heterophyllum benth, comprising the following steps:
first extraction
Drying the dracocephalum heterophyllum benth in the shade, crushing, adding an ethanol solution with the volume concentration of 95% and the mass of 8 times of that of the dracocephalum heterophyllum benth, soaking for 10 hours, heating and refluxing at 80 ℃ for 2 times, and extracting for 3 hours each time to obtain an extracting solution, and drying the extracting solution under reduced pressure to obtain a paste, namely the dracocephalum heterophyllum benth plant alcohol extract.
wherein: the reduced pressure drying condition means that the vacuum degree is 0.09 MPa and the temperature is 50 ℃.
Secondly, liquid and liquid distribution and enrichment:
Dispersing 1.0 Kg of the dracocephalum heterophyllum plant alcohol extract with 30 times of analytical pure water to obtain dispersion, extracting the dispersion with 30 times of ethyl acetate for 3 times, and mixing to obtain ethyl acetate extract; the ethyl acetate extract was dried under reduced pressure to obtain 162.1 g of the medium polar group of Dracocephalum heterophyllum.
Wherein: the reduced pressure drying condition means that the vacuum degree is 0.09 MPa and the temperature is 50 ℃.
Removing impurities by using microporous resin:
Dissolving the medium-polarity component parts of the dracocephalum heterophyllum benth with a methanol solution with 5 times of the mass and 90% of volume fraction, filtering to obtain a filtrate, separating the filtrate on a microporous resin column, eluting with a methanol solution with 3 times of the column volume and 90% of volume fraction, and collecting the 90% methanol solution eluate; vacuum drying 90% methanol solution eluate to obtain yellow crude product of flavonoid component of Dracocephalum heterophyllum 104.6 g.
Wherein: microporous resin refers to HP20SS type resin column.
The proportion of the medium-polarity component part of the dracocephalum heterophyllum benth to the microporous resin is 1 g: 30 mL.
the reduced pressure drying condition means that the vacuum degree is 0.09 MPa and the temperature is 50 ℃.
Fourth, silica gel column chromatography separation:
Separating the crude flavonoid component of the dracocephalum heterophyllum benth by silica gel column chromatography, eluting with a chloroform-methanol mixed solvent with 5 times of column volume, collecting fractions with the volume of 500 mL per fraction, and detecting by adopting thin layer chromatography, wherein the developing solvent is chloroform and methanol, and the weight ratio of the developing solvent is 5: 5 (mL/mL), and the color developing agent is concentrated sulfuric acid ethanol solution with the volume concentration of 10%, and fractions with the Rf value of 0.1-0.8 are combined and collected, and are dried under reduced pressure to obtain 48.0 g of yellow powdery isolobate bluish flavonoid component.
Wherein: the size of the silica gel column was 40 mm × 60 cm.
The chloroform-methanol mixed solvent refers to chloroform and methanol according to the ratio of 3: 7 (mL/mL) in a volume ratio.
The reduced pressure drying condition means that the vacuum degree is 0.09 MPa and the temperature is 50 ℃.
Embodiment 2 a method for preparing flavonoid components from dracocephalum heterophyllum benth, comprising the following steps:
first extraction
Drying the dracocephalum heterophyllum benth in the shade, crushing, adding a methanol solution with the volume concentration of 95% and the mass of 20 times of that of the dracocephalum heterophyllum benth, soaking for 15 hours, heating and refluxing at 90 ℃ for 4 times, and extracting for 3 hours each time to obtain an extracting solution, and drying the extracting solution under reduced pressure to obtain a paste, namely the dracocephalum heterophyllum benth plant alcohol extract.
wherein: the reduced pressure drying condition means that the vacuum degree is 0.06MPa and the temperature is 70 ℃.
Secondly, liquid and liquid distribution and enrichment:
dispersing 5.0 Kg of the dracocephalum heterophyllum plant alcohol extract with 50 times of analytical pure water to obtain dispersion, extracting the dispersion with 50 times of ethyl acetate for 3 times, and mixing to obtain ethyl acetate extractive solution; the ethyl acetate extract is dried under reduced pressure to obtain 822.4 g of medium polarity group of dracocephalum heterophyllum.
wherein: the reduced pressure drying condition means that the vacuum degree is 0.06MPa and the temperature is 70 ℃.
Removing impurities by using microporous resin:
Dissolving the medium-polarity component parts of the dracocephalum heterophyllum benth with a methanol solution with the volume fraction of 80% and the mass of the component parts being 10 times that of the dracocephalum heterophyllum benth, filtering to obtain a filtrate, separating the filtrate on a microporous resin column, eluting with a methanol solution with the volume fraction of 80% and the volume of 5 times that of the column, and collecting the eluate of the methanol solution with the volume fraction of 80%; and (3) drying the eluate in 80% methanol solution under reduced pressure to obtain 522.4 g of yellow crude flavonoid component of the dracocephalum heterophyllum.
wherein: the microporous resin refers to MCI type resin column.
the proportion of the medium-polarity component part of the dracocephalum heterophyllum benth to the microporous resin is 1 g: 30 mL.
the reduced pressure drying condition means that the vacuum degree is 0.06MPa and the temperature is 70 ℃.
Fourth, silica gel column chromatography separation:
Separating the crude flavonoid component of the dracocephalum heterophyllum benth by silica gel column chromatography, eluting with 10 times column volume of chloroform-methanol mixed solvent, collecting the fraction with each 1000 mL, and detecting by thin layer chromatography, wherein the developing solvent is chloroform and methanol, and the ratio of the developing solvent to the total flavonoid component is 5: 5 (mL/mL), and the color developing agent is concentrated sulfuric acid ethanol solution with the volume concentration of 10%, and fractions with the Rf value of 0.1-0.8 are combined and collected, and are dried under reduced pressure to obtain 236.8 g of yellow powdery isolobate bluish flavonoid component.
Wherein: the size of the silica gel column was 80 mm × 100 cm.
The chloroform-methanol mixed solvent refers to chloroform and methanol according to the ratio of 7: 3 (mL/mL) in a volume ratio.
The reduced pressure drying condition means that the vacuum degree is 0.06MPa and the temperature is 70 ℃.
Embodiment 3 a method for preparing flavonoid components from dracocephalum heterophyllum benth, comprising the following steps:
First extraction
drying the dracocephalum heterophyllum benth in the shade, crushing, adding a 95% ethanol solution with the volume concentration of 14 times of the weight of the dracocephalum heterophyllum benth, soaking for 12 hours, heating and refluxing at 85 ℃ for 3 times, extracting for 3 hours each time to obtain an extracting solution, and drying the extracting solution under reduced pressure to obtain a paste to obtain the dracocephalum heterophyllum benth plant alcohol extract.
Wherein: the reduced pressure drying condition means that the vacuum degree is 0.08 MPa and the temperature is 60 ℃.
Secondly, liquid and liquid distribution and enrichment:
2.0 Kg of the dracocephalum heterophyllum plant alcohol extract is dispersed by analytical pure water with the mass 40 times of that of the dracocephalum heterophyllum plant alcohol extract to obtain dispersion liquid, the dispersion liquid is extracted by ethyl acetate with the volume 40 times of that of the dispersion liquid for 3 times, and ethyl acetate extraction liquid is obtained by combination; the ethyl acetate extract is dried under reduced pressure to obtain 318.6 g of medium polarity group of dracocephalum heterophyllum.
wherein: the reduced pressure drying condition means that the vacuum degree is 0.08 MPa and the temperature is 60 ℃.
Removing impurities by using microporous resin:
dissolving the medium-polarity component parts of dracocephalum heterophyllum with a methanol solution with a volume fraction of 85% and 8 times of the mass of the component parts, filtering to obtain a filtrate, separating the filtrate on a microporous resin column, eluting with a methanol solution with a volume fraction of 85% and 4 times of the column volume, and collecting the eluate of the methanol solution with a volume fraction of 85%; and (3) drying the eluate in 85% methanol solution under reduced pressure to obtain 198.2 g of yellow crude flavonoid component of the dracocephalum heterophyllum.
Wherein: microporous resin refers to HP20SS type resin column.
The proportion of the medium-polarity component part of the dracocephalum heterophyllum benth to the microporous resin is 1 g: 30 mL.
The reduced pressure drying condition means that the vacuum degree is 0.08 MPa and the temperature is 60 ℃.
fourth, silica gel column chromatography separation:
Separating the crude flavonoid component of the dracocephalum heterophyllum benth by silica gel column chromatography, eluting with a chloroform-methanol mixed solvent with the volume of 8 times of the column volume, collecting the fraction of 800 mL of each fraction, and detecting by adopting thin-layer chromatography, wherein the developing solvent is chloroform and methanol, and the ratio of the developing solvent to the total flavonoid component is 5: 5 (mL/mL), and the color developing agent is concentrated sulfuric acid ethanol solution with the volume concentration of 10%, and fractions with the Rf value of 0.1-0.8 are combined and collected, and are dried under reduced pressure to obtain 88.6 g of yellow powdery isolobate bluish flavonoid component.
Wherein: the size of the silica gel column is 50 mm × 80 cm.
A chloroform-methanol mixed solvent means chloroform and methanol in a ratio of 5: 5 (mL/mL) in a volume ratio.
The reduced pressure drying condition means that the vacuum degree is 0.08 MPa and the temperature is 60 ℃.
The application of the flavonoid component of dracocephalum heterophyllum prepared in the above examples 1-3 in preparing anti-hepatitis virus drugs or health food is as follows: the flavonoid component of the dracocephalum heterophyllum benth can be used as an effective component to prepare various anti-hepatitis virus medicinal preparations with any pharmaceutically acceptable carrier by a conventional method, or can be used as an effective component to prepare various health-care foods with any pharmaceutically acceptable carrier by a conventional method.
Claims (6)
1. A method for preparing flavonoid components of dracocephalum heterophyllum benth comprises the following steps:
first extraction
Drying and crushing the dracocephalum heterophyllum benth plant in the shade, adding an ethanol or methanol solution with the volume concentration of 95% and the mass of 8-20 times of that of the dracocephalum heterophyllum benth plant, soaking for 10-15 hours, heating and refluxing for 2-4 times at 80-90 ℃, extracting for 3 hours each time to obtain an extracting solution, and drying the extracting solution under reduced pressure to obtain a paste, namely the dracocephalum heterophyllum benth plant alcohol extract;
Secondly, liquid and liquid distribution and enrichment:
Dispersing the dracocephalum heterophyllum plant alcohol extract by using 30-50 times of analytical pure water by mass to obtain dispersion liquid, extracting the dispersion liquid for 3 times by using 30-50 times of ethyl acetate by volume, and combining to obtain ethyl acetate extract; the ethyl acetate extract is dried under reduced pressure to obtain the medium-polarity component part of the dracocephalum heterophyllum;
Removing impurities by using microporous resin:
Dissolving the medium-polarity component parts of the dracocephalum heterophyllum benth with a methanol solution with the mass of 5-10 times and the volume fraction of 80-90%, filtering to obtain a filtrate, separating the filtrate on a microporous resin column, eluting with a methanol solution with the volume fraction of 3-5 times and the volume fraction of 80-90%, and collecting the eluate of the methanol solution with the volume fraction of 80-90%; decompressing and drying the eluate of the 80-90% methanol solution to obtain a yellow crude product of the flavonoid component of the dracocephalum heterophyllum; the proportion of the medium-polarity component part of the dracocephalum heterophyllum benth to the microporous resin is 1 g: 30 mL;
Fourth, silica gel column chromatography separation:
Separating the crude flavonoid component of the dracocephalum heterophyllum benth by silica gel column chromatography, eluting with a chloroform-methanol mixed solvent with the volume of 5-10 times of the column volume, collecting fractions according to 500-1000 mL of each fraction, and detecting by adopting thin-layer chromatography, wherein a developing agent is chloroform and methanol, and the ratio of chloroform to methanol is 5: 5, the color developing agent is concentrated sulfuric acid ethanol solution with volume concentration of 10%, fractions with Rf value of 0.1-0.8 are merged and collected, and the fractions are dried under reduced pressure to obtain yellow powdery flavonoid components of the dracocephalum heterophyllum benth.
2. The method for preparing the flavonoid component of Dracocephalum heterophyllum according to claim 1, wherein the flavonoid component is prepared by the following steps: the reduced pressure drying condition is that the vacuum degree is 0.06-0.09 MPa and the temperature is 50-70 ℃.
3. The method for preparing the flavonoid component of Dracocephalum heterophyllum according to claim 1, wherein the flavonoid component is prepared by the following steps: the microporous resin in the step three is an HP20SS type resin column or an MCI type resin column.
4. The method for preparing the flavonoid component of Dracocephalum heterophyllum according to claim 1, wherein the flavonoid component is prepared by the following steps: the size of the silica gel column in the step four is 40 mm-80 mm multiplied by 60 cm-100 cm.
5. the method for preparing the flavonoid component of Dracocephalum heterophyllum according to claim 1, wherein the flavonoid component is prepared by the following steps: the chloroform-methanol mixed solvent in the step four is a mixture of chloroform and methanol in a ratio of 7: 3-3: 7 by volume ratio.
6. the use of the flavonoid component of Dracocephalum heterophyllum as claimed in claim 1 in the preparation of anti-hepatitis virus drugs or health foods, wherein the flavonoid component of Dracocephalum heterophyllum is prepared by the method comprising the following steps: the flavonoid component of the dracocephalum heterophyllum benth can be used as an effective component to prepare various anti-hepatitis virus medicinal preparations with any pharmaceutically acceptable carrier by a conventional method, or can be used as an effective component to prepare various health-care foods with any pharmaceutically acceptable carrier by a conventional method.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102078374A (en) * | 2009-11-29 | 2011-06-01 | 李红玉 | Tibetan medical dracocephalum heterophyllum benth extract and application thereof |
| CN103070916A (en) * | 2013-01-25 | 2013-05-01 | 中国科学院新疆理化技术研究所 | Preparation method and application of effective part of dracocephalum heterophyllum benth |
| CN103463182A (en) * | 2013-08-26 | 2013-12-25 | 兰州大学 | Preparation method and application of dracocephalum heterophyllum benth fractionated extracts |
| CN104151390A (en) * | 2014-08-06 | 2014-11-19 | 中国科学院西北高原生物研究所 | Method for separating and preparing ursolic acid methyl ester from dracocephalum heterophyllum benth and application of ursolic acid methyl ester |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102078374A (en) * | 2009-11-29 | 2011-06-01 | 李红玉 | Tibetan medical dracocephalum heterophyllum benth extract and application thereof |
| CN103070916A (en) * | 2013-01-25 | 2013-05-01 | 中国科学院新疆理化技术研究所 | Preparation method and application of effective part of dracocephalum heterophyllum benth |
| CN103463182A (en) * | 2013-08-26 | 2013-12-25 | 兰州大学 | Preparation method and application of dracocephalum heterophyllum benth fractionated extracts |
| CN104151390A (en) * | 2014-08-06 | 2014-11-19 | 中国科学院西北高原生物研究所 | Method for separating and preparing ursolic acid methyl ester from dracocephalum heterophyllum benth and application of ursolic acid methyl ester |
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| Title |
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| 藏药异叶青兰的黄酮成分;张德等;《青海师范大学学报(自然科学版)》;19970715(第03期);第47-50页 * |
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